超高效液相色谱-串联质谱法同时检测溴代阻燃剂

摘要

采用Acquity BEH C18色谱柱,以甲醇-乙腈混合液和水为流动相,辅以电喷雾正离子模式多反应监测(MRM)进行定性定量分析,建立了一种同位素稀释超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测四溴双酚A(TBBPA)、三-(2,3-二溴丙基)异氰脲酸酯(TBC)和3种六溴环十二烷(HBCD)异构体的方法.水样通过固相萃取进行净化,回收率达到85.3％ ～96.1％.土壤和底泥样品经加速溶剂萃取后,采用酸性硅胶和中性硅胶柱进行净化,回收率达到81.5％～102.7％.谊方法对TBBPA、TBC、α-HBCD、β-HBCD、γ-HBCD在水和土壤中的检测限分别为1.0、1.2、2.0、0.8、1.2 ng/L和0.10、0.12、0.20、0.08、0.12 ng/g.%A sensitive and selective method was developed for simultaneous analysis tetrabromobisphenol A (TBBPA),tris-(2,3-dibromopropyl) isocyanurate(TBC) and hexabromocyclododecanes (HBCD) in water,soil and sediment samples.The method included an Acquity BEH C18 column separation operated with a gradient elution solvent of methanol-acetonitrile and water coupled to a mass Spectrometry scanned in multiple reaction monitoring (MRM) mode and isotope dilution.Water samples were extracted and cleaned-up by solid phase extraction.The recoveries were in the range of 85.3％-96.1％.Soil and sediment samples were extracted using accelerated solvent extraction (ASE),and further purified using acidic silica treatment and solid phase extraction with an activated silica gel column.The recoveries in soil and sediment samples were 81.5％-102.7％.Limits of detection of TBBPA,TBC,α-HBCD,β-HBCD,γ-HBCD were 1.0,1.2,2.0,0.8,1.2 ng/L in water samples and 0.10,0.12,0.20,0.08,0.12 ng/g in soil and sediment samples,respectively.